MYSTAT: A compact potentiostat/galvanostat for general electrochemistry measurements.

An open-source potentiostat/galvanostat instrument design is introduced that provides the ability to take accurate measurements over a current range of ±200 mA and a potential range of ±12 V. The improved capability of the instrument compared to the previously published design upon which it is based makes it suitable for performing a wider range of electrochemical measurements including the ability to use larger working electrodes, study of high current density processes, study of electrochemistry in nonaqueous solutions and use in high voltage processes such as electrophoretic deposition. The instrument can be controlled from any computer capable of running the Python programming language, including a low-cost Raspberry Pi. Unlike many commercial potentiostat designs, the instrument is completely open-source, giving researchers the ability to modify the hardware and software as needed for custom measurement techniques. The low cost makes the instrument attractive for research and teaching laboratories in which multiple electrochemical measurements need to be carried out in parallel.

Steric stabilization of thermally responsive N-isopropylacrylamide particles by poly(vinyl alcohol).

Poly(vinyl alcohol) (PVA) was used as a steric stabilizer for the dispersion polymerization of cross-linked poly(N-isopropylacrylamide) (PNIPAM) in water. A series of reactions were carried out using PVA of varying molecular weight and degree of hydrolysis. Under appropriate conditions, PNIPAM particles of uniform and controllable size were produced using PVA as the stabilizer. The colloidal stability was investigated by measuring changes in particle size with temperature in aqueous suspensions of varying ionic strength. For comparison, parallel colloidal stability measurements were conducted on PNIPAM particles synthesized with low-molecular-weight ionic surfactants. PVA provides colloidal stability over a wide range of temperature and ionic strength, whereas particles produced with ionic surfactants flocculate in moderate ionic strength solutions upon collapse of the hydrogel as the temperature is increased. Experimental results and theoretical consideration indicate that sterically stabilized PNIPAM particles resulted from the grafting of PVA to the PNIPAM particle surface. The enhanced colloidal stability afforded by PVA allows the temperature-responsive PNIPAM particles to be used under physiological conditions where electrostatic stability is ineffective.

Encapsulation and sustained release from biodegradable microcapsules made by emulsification/freeze drying and spray/freeze drying.

Hollow biodegradable poly(DL-lactide) (PLA) particles with porous shell walls were prepared by freeze drying small droplets of PLA solution formed by emulsification or spraying. The hollow freeze-dried particles were dispersed in water, and the resulting aqueous suspensions were exposed to plasticizing solvents, either dichloromethane or compressed carbon dioxide. The plasticizing solvent causes the pores in the shell wall to close, forming microcapsules surrounding an aqueous core. A water soluble drug, procaine hydrochloride, was successfully encapsulated in the microcapsule core. The encapsulation efficiency is affected by the hollow particle morphology, amount of solvent used, solvent exposure time, surfactant, and method of dispersing the freeze-dried particles in water. The encapsulation process is explained in terms of interfacial free energy of the hollow particles and mobility of the plasticized polymer. Controlled release of procaine hydrochloride from the microcapsules into phosphate buffer solution was observed. The microcapsules had a small burst release, with the remainder of encapsulated drug slowly released over 9 days. The novel hollow PLA particles produced by emulsification/freeze drying and spray/freeze drying can potentially be used as vehicles for controlled release.

Effect of interfacial free energy on the formation of polymer microcapsules by emulsification/freeze-drying.

Hollow polymer microparticles with a single opening on the surface were formed by freeze-drying aqueous polymer colloids swollen with solvent. The results show that the particle morphology is due to phase separation in the polymer emulsion droplets upon freezing in liquid nitrogen, and that morphological changes are driven largely by lowering interfacial free energy. The effects of added surfactant, volume fraction of solvent, type of solvent, and processing conditions on the particle morphology were examined and compared to theoretical predictions. The dried hollow particles were resuspended in a dispersing media and exposed to a second swelling solvent to close the surface opening and form microcapsules. The interfacial free energy difference between the inside and outside surfaces is the driving force for closing the hole on the surface. The emulsification/freeze-drying technique can be used to encapsulate hydrophilic additives in the core of the microcapsules, demonstrating the potential of the technique in controlled-release applications.

Altering the crystal morphology of silicalite-1 through microemulsion-based synthesis.

The crystal morphology of silicalite-1 was adjusted through a microemulsion-based hydrothermal synthesis. The surfactant cetyltrimethylammonium bromide (CTAB) with cosurfactant butanol was used to form water-in-oil microemulsions containing the silicalite-1 synthesis gel. The crystal morphology of silicalite-1 was adjusted from coffin-shaped to novel rod-shaped and to irregular-shaped nanoparticles by varying the microemulsion composition. Silicalite-1 synthesized in the microemulsion has a smaller size and a more narrow size distribution than that produced by conventional synthesis without the microemulsion. The novel morphology of silicalite-1 may facilitate assembly into films and find applications in separation and catalysis.

Encapsulation and sustained release of a model drug, indomethacin, using CO(2)-based microencapsulation.

A carbon dioxide (CO(2))-based microencapsulation technique was used to impregnate indomethacin, a model drug, into biodegradable polymer nanoparticles. Compressed CO(2) was emulsified into aqueous suspensions of biodegradable particles. The CO(2) plasticizes the biodegradable polymers, increasing the drug diffusion rate in the particles so that drug loading is enhanced. Four types of biodegradable polymers were investigated, including poly(d,l-lactic acid) (PLA), poly(d,l-lactic acid-co-glycolic acid) (PLGA) with two different molar ratios of LA to GA, and a poly(d,l-lactic acid-b-ethylene glycol) (PLA-PEG) block copolymer. Biodegradable nanoparticles were prepared from polymer solutions through nonsolvent-induced precipitation in the presence of surfactants. Indomethacin was incorporated into biodegradable nanoparticles with no change of the particle size and morphology. The effects of a variety of experimental variables on the drug loadings were investigated. It was found that the drug loading was the highest for PLA homopolymer and decreased in PLGA copolymers as the fraction of glycolic acid increased. Indomethacin was predicted to have higher solubility in PLA than in PLGA based on the calculated solubility parameters. The drug loading in PLA increased markedly as the temperature for impregnation was increased from 35 to 45 degrees C. Drug release from the particles is a diffusion-controlled process, and sustained release can be maintained over 10 h. A simple Fickian diffusion model was used to estimate the diffusion coefficients of indomethacin in the biodegradable polymers. The diffusion coefficients are consistent with previous studies, suggesting that the polymer properties are unchanged by supercritical fluid processing. Supercritical CO(2) is nontoxic, easily separated from the polymers, can extract residual organic solvent, and can sterilize biodegradable polymers. The CO(2)-based microencapsulation technique is promising for the production of drug delivery devices without the use of harmful solvents.